Lead compounds of 4:6-dinitroresorcinol

ABSTRACT

THE INVENTION RELATES TO LEAD COMPOUNDS 4:6-DINITRORESORCINOL WHICH MAY BE USED AS PRIMING AND FAST DELAY COMPOSITIONS FOR FUSES AND DETONATORS. HITHERTO LEAD COMPOUNDS OF 4:6-DINITROESORCINOL HAVE HAD LIMITED TECHNICAL APPLICATION BECAUSE OF THE DIFFICULTY IN PREPARING THEM IN REPRODUCIBLE AND FREE-FLOWING FORM. FURTHERMORE, THESE COMPOUNDS OFTEN APPEAR TO BE OF INDEFINITE CONSTITUTION AND, BECAUSE OF THEIR INSOLUBLE NATURE, THEY ARE PRECIPITATED IN VERY FINELY DIVIDED FORM TO GIVE A PRODUCT WHICH CAKES ON DRYING AND IS OF LOW BULK DENSITY, DUSTY AND POOR FLOWING.

- ammonium hydroxide are preferred in United States Patent Patented Aims, 1974' ABSTRACT OF THE DISCLOSURE The invention relates to lead compounds of 4:6-dinitroresorcinol which may be used as priming ilnd fast delay compositions for fuses and detonators. Hitherto lead compounds of 4:6-dinitrorcsorcinol have had limited technical application because of the difliculty in preparing them in reproducible and free-flowing form. Furthermore, these. 1 compounds often appear to be of indefinite constitution and, because of their inso1u ble, nature, they are precipitated in very finely divided form to give a product which cakes on drying-and is of low bulk density, dusty and poor flowing.

The present invention provides a new lead compound 01' 4:6-dinitroresorcinol, which may be prepared in a reproducible'form having a high bulk density and which is frec-flowing. dust-free and very suitable for technical use in primers, fuses and detonators. 1

The new compound has the formula 3[c,H,N,o.pbi2[Pb oma corresponding to the stoichiometric proportions 3(norma1 lead 4:6-dinitroresorcinate)2(1ead hydroxide) and is prepared by intcrmixing a water-soluble lead salt and an alkaline hydroxidwwith 4:6-dinitrorcsorcinol at an elevated temperature. The process is preferably carried out by the addition of a water-soluble lead salt and an alkaline hydroxide to a suspension of finely divided 4:6-dinitroresorcinol. The temperature of the reaction mixture is preferably maintained between about, 70 and 100 C. The

relative proportions of 416-dinitroresorcino and 'lead salt employed should approximate to the stoiehiometric requirements of the ahoye formula. Any solublelead salt or alkaline hydroxide may beused but lead acetate and order to give' a product of high bulk density. t l I v By way of example, atypical process for themanufac: ture of the new compound in accordance with the invention will now be described.

600 g. of finely divided 4:6-dinitroi'esoreino1 is suspended with stirring in 35 litres of water in 50 litres stainless steel pan jacketed for steam and cold water circulation. The temperature is raised to (7. and then 7.25

. litres vat- 1.5 N lead acetate solution and 7.25 1itres of 1.15

N ammonium hydroxide solution are added simultane 'ously during 95-105 minutes. The temperature 18 matntaincd at. 90 C. for a "further minutes, and then rev d'uccd to C. by cold water circulation through the pun jacket. Stirring is then stopped and the product allowcd'to settle for 3 minutes before decantationof the .mother liquor. It is then. washed with} successive 20 litre portions ofbwater with 3 minutes stirring and} minutes ,settling,'in each wash, and transferred to a filter where i it is finally washed with Z-litres of industrial methylated spirits. Drying is effected by passage of cold air or one hot-table at C., andthe product may then be passed through a 50 13.5.5. mesh sieve, leaving little orno oversize. T

" The yield is 1650 g. 4.96 percent theoretical.) of a free .Lflowing; granular product having a bulk density 1.4 g./ml.

Analysis ofth e product gives Pb 60.9'; dinitroresorcinol 34.8;carbon 12.74)? (theoretical: 61.0; 35.0; 12.73%). This material is especially suitable as a fast-burning delay composition and as an ingredient oft-an igniting contposition.

We claim: 1 t

v 1. A Method of producing a chemical compound in which three portions of lead 4:6-dinitroresorcinatc are bonded to two portions of lead hydroxide, which consists of reacting a water soluble'leadsalt'and an alkaline hydroxidc with 41o-dinilroresoreiuel; said reactants being brought together in the s'toichiometric quantities required by the product.

2. A process according to claim 1 whichiscarried out at a temperature between and C. 4 t

- 3.. A process according to claim l whereiu the lead salt is lead acetate.

r 4. A process according to claim 1 wherein the alkaline hydroxide is ammoniumhydroxide. t

' 5. A leadcompound of 4:6-dinitroresorcino1 having a formula corresponding" to the stoichiometric proportions .3(normal lead 4z6-dinitrorcsorcinatc')2(lead hydroxide).

References (lited v I UNITED STATES PATENTS 2,441,248 f 5/1948 Morris et a1. 149 -'-=25X ,LELAND A. SEBASTIAN, Primary Examiner Us. C1. e-R. 

